[go: up one dir, main page]

EP0946458A1 - Procede de fabrication d'un materiau composite ceramique - Google Patents

Procede de fabrication d'un materiau composite ceramique

Info

Publication number
EP0946458A1
EP0946458A1 EP97936901A EP97936901A EP0946458A1 EP 0946458 A1 EP0946458 A1 EP 0946458A1 EP 97936901 A EP97936901 A EP 97936901A EP 97936901 A EP97936901 A EP 97936901A EP 0946458 A1 EP0946458 A1 EP 0946458A1
Authority
EP
European Patent Office
Prior art keywords
composite material
reinforcing
matrix
immersed
interface
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP97936901A
Other languages
German (de)
English (en)
Other versions
EP0946458B1 (fr
Inventor
Robert Lundberg
Magnus Holmquist
Anthony Gordon Razzell
Ludovic Molliex
Olivier Sudre
Michel Parlier
Fabrice Rossignol
Julien Parmentier
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Office National dEtudes et de Recherches Aerospatiales ONERA
Safran Aircraft Engines SAS
Rolls Royce PLC
GKN Aerospace Sweden AB
Original Assignee
Office National dEtudes et de Recherches Aerospatiales ONERA
Societe Nationale dEtude et de Construction de Moteurs dAviation SNECMA
SNECMA SAS
Rolls Royce PLC
Volvo Aero AB
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Office National dEtudes et de Recherches Aerospatiales ONERA, Societe Nationale dEtude et de Construction de Moteurs dAviation SNECMA, SNECMA SAS, Rolls Royce PLC, Volvo Aero AB filed Critical Office National dEtudes et de Recherches Aerospatiales ONERA
Publication of EP0946458A1 publication Critical patent/EP0946458A1/fr
Application granted granted Critical
Publication of EP0946458B1 publication Critical patent/EP0946458B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844Coating fibres
    • C04B35/62857Coating fibres with non-oxide ceramics
    • C04B35/62873Carbon
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/111Fine ceramics
    • C04B35/117Composites
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844Coating fibres
    • C04B35/62847Coating fibres with oxide ceramics
    • C04B35/62855Refractory metal oxides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62892Coating the powders or the macroscopic reinforcing agents with a coating layer consisting of particles
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62894Coating the powders or the macroscopic reinforcing agents with more than one coating layer
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62897Coatings characterised by their thickness
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • C04B35/645Pressure sintering
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/522Oxidic
    • C04B2235/5224Alumina or aluminates

Definitions

  • the present invention refers to a method of manufacturing a ceramic composite material comprising matrix and reinforcing materials and an intermediate weak interface material, said composite material being particularly intended for use at temperatures above 1400°C and in an oxidizing environment, the matrix and reinforcing materials consisting of the same or dif- ferent ceramic oxides having a melting point above 1600°C, and the interface material providing in combination with said materials a stress field liable to micro-cracking.
  • the main object of the present invention is to suggest a method by which an even weaker interface is obtained.
  • the reinforcing fibre material is immersed into a powder slurry containing carbon and Zr0 2 so as to be coated thereby and then dried, after which the composite material is subjected to green forming and densification steps as known per se, and finally a heat-treatment in air leaving a porous structure of the interface material.
  • the reinforcing fibre material is immersed into and coated with a first powder slurry contain- ing Zr0 2 and then- dried and immersed into and .
  • the coating formed on fibres of which the reinforcing material consist and which are immersed in the slurry has proved to be adherent and strong enough to survive green forming and densification processes.
  • the C is removed by heat treatment in air, leaving a gap or porosity in the oxide interface.
  • the volume fraction of C can be varied to achieve the desired interface strength.
  • the interface made by this invention is stable at high temperatures for long times because the pores have got the right size, i.a. are large enough .
  • the re- inforcement is first immersed in a C powder slurry, dried and then immersed in an oxide (Zr0 2 ) powder slurry, forming a double . or sequential coating. Again, this coating is strong and adherent enough to survive green forming and densification. After densification the C is removed by heat treatment leaving a gap between the reinforcing material and the oxide interface. Surface roughness of the reinforcing and matrix materials is sufficient to give load transfer between reinforcing material and matrix materia-1.
  • the absence of bonding between the oxide interface and the reinforcing material will ensure effective crack deflection.
  • the degree of load transfer and frictional sliding resistance between reinforcing material and matrix con- trolling the fibre pullout behaviour can be varied by varying the thickness of the fugitive C layer.
  • Example 1 Single crystal fibres of Al 2 0 3 (from Saphikon Inc., USA) were covered with a thin layer of C/Zr0 2 mixture. This was made by immersing the fibres in a slurry of C/Zr0 2 -powder in water. The volume proportions of C to Zr0 2 was 1/1. After drying the coated fibres were stacked to a fibre preform in a plaster mould. A Al 2 0 3 powder slurry was poured thereon and a pressure gradient was applied to give good infiltration of the fibre preform.
  • Example 1 was repeated however using Hf0 2 instead of Zr0 2 .
  • Example 3 Single crystal fibres of Al 2 0 3 (from Saphikon Inc., USA) were covered with at thin double layer of C and Zr0 2 . This was made by first immersing the fibres in a slurry of Zr0 2 -powder in water and then immersing the fibres in a slurry of C-powder in water. After drying the coated fibres were stacked to a fibre preform in a plaster mould. An Al 2 0 3 powder slurry was poured thereon and a pressure gradient was applied to give good infiltration of the fibre preform.
  • the green bodies were sintered by hot- pressing at 1400°C, at 10 MPa for 70 minutes.
  • the C was burnt out by heat treatment at 1250°C for 10 hours leaving a gap of about 1 ⁇ m between the zirconia layer and the Al 2 0 3 matrix.
  • the Zr0 2 layer was about 3 ⁇ m of thickness and not bonded to the matrix.
  • the gap between fibre and Zr0 2 layer provided crack deflection and fibre pullout which was proved by bending tests.
  • Example 4 Example 3 was repeated however using Hf0 2 instead of Zr0 2 .
  • Example 5 - Example 3 was repeated, however with the steps in slightly reversed order, i.e. by first immersing the fibres in a slurry of C-powder in water and then in a slurry of Zr0 2 - powder, with similar advantageous result.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Ceramic Products (AREA)

Abstract

L'invention porte sur un procédé de fabrication d'un matériau composite céramique comprenant une matrice, des matériaux de renfort, et un matériau interface faible. Ledit matériau composite est particulièrement adapté aux températures supérieures à 1400 °C et aux atmosphères oxydantes. La matrice et les matériaux de renfort sont en oxydes céramiques identiques ou différents, d'un point de fusion supérieur à 1600 °C, et le matériau interface fournit, en association avec les autres matériaux, un champ de contraintes susceptible de microcraquelures. Selon l'invention, le matériau fibreux de renfort est plongé dans une boue pulvérulente contenant du carbone (C) et du ZrO2 dont il s'imprègne, puis séché. Il est ensuite transformé en pâte verte puis soumis à des étapes de densification connues per se, puis finalement à un traitement thermique laissant une structure poreuse sur le matériau interface.
EP97936901A 1997-08-11 1997-08-11 Procede de fabrication d'un materiau composite ceramique Expired - Lifetime EP0946458B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/SE1997/001340 WO1999007653A1 (fr) 1997-08-11 1997-08-11 Procede de fabrication d'un materiau composite ceramique

Publications (2)

Publication Number Publication Date
EP0946458A1 true EP0946458A1 (fr) 1999-10-06
EP0946458B1 EP0946458B1 (fr) 2001-11-28

Family

ID=20406529

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97936901A Expired - Lifetime EP0946458B1 (fr) 1997-08-11 1997-08-11 Procede de fabrication d'un materiau composite ceramique

Country Status (7)

Country Link
US (1) US6251317B1 (fr)
EP (1) EP0946458B1 (fr)
JP (1) JP2001502290A (fr)
CA (1) CA2268019C (fr)
DE (1) DE69708682T2 (fr)
ES (1) ES2164364T3 (fr)
WO (1) WO1999007653A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7105224B2 (en) 2001-11-23 2006-09-12 Fraunhofer-Gesellschaft Zur Foerderung Der Angewandten Forschung E.V. Oxide ceramic fiber composite materials and use thereof

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2778655B1 (fr) * 1998-05-15 2000-08-11 Aerospatiale Procede d'elaboration d'un materiau d'interphase, materiau obtenu, procede de traitement d'une fibre ceramique de renfort avec ce materiau et materiau thermostructural incluant de telles fibres
EP2181974B1 (fr) * 2008-10-31 2012-03-21 AVIO S.p.A. Procédé pour la production de composants fabriqués à partir d'un matériau composite à matrice céramique
US8309197B2 (en) * 2008-12-17 2012-11-13 Teledyne Scientific & Imaging, Llc Integral abradable seals
GB201006625D0 (en) 2010-04-21 2010-06-02 Rolls Royce Plc A method of manufacturing a ceramic matrix composite article
FR3041890B1 (fr) * 2015-10-05 2017-11-24 Snecma Procede de fabrication d'une piece en materiau composite par injection d'une barbotine chargee dans un moule poreux
JP7187369B2 (ja) 2019-03-25 2022-12-12 三菱重工航空エンジン株式会社 セラミックス基複合材料の製造方法
US11787746B1 (en) * 2021-02-10 2023-10-17 Hrl Laboratories, Llc Compressible coating reinforcements for ceramic matrix composites, and methods of making the same
CN118812268B (zh) * 2024-07-24 2025-10-28 哈尔滨工业大学 一种C/ZrO2复合涂层改性纤维莫来石先驱体的制备方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4732877A (en) 1985-09-30 1988-03-22 Allied-Signal Inc. Alumina composite reinforced by zirconia-clad alumina fibers
US4885199A (en) * 1986-08-06 1989-12-05 Norton Company Fiber-reinforced silicon nitride composite ceramics
US5290491A (en) 1990-04-02 1994-03-01 Societe Europeenne De Propulsion Process for the manufacture of a thermostructural composite material having a carbon interphase between its reinforcement fibers and its matrix
FR2685693B1 (fr) * 1991-12-30 1994-06-03 Europ Propulsion Procede de realisation d'une protection contre l'oxydation de produits en materiau composite, et produits ainsi proteges.

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9907653A1 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7105224B2 (en) 2001-11-23 2006-09-12 Fraunhofer-Gesellschaft Zur Foerderung Der Angewandten Forschung E.V. Oxide ceramic fiber composite materials and use thereof

Also Published As

Publication number Publication date
CA2268019A1 (fr) 1999-02-18
US6251317B1 (en) 2001-06-26
ES2164364T3 (es) 2002-02-16
DE69708682T2 (de) 2002-08-08
EP0946458B1 (fr) 2001-11-28
DE69708682D1 (de) 2002-01-10
WO1999007653A1 (fr) 1999-02-18
JP2001502290A (ja) 2001-02-20
CA2268019C (fr) 2007-03-13

Similar Documents

Publication Publication Date Title
Chartier et al. Laminar ceramic composites
Plucknett et al. Processing of Tape–Cast Laminates Prepared from Fine Alumina/Zirconia Powders
US5866244A (en) Ceramic structure with backfilled channels
EP0946458B1 (fr) Procede de fabrication d'un materiau composite ceramique
US5856252A (en) Damage tolerant ceramic matrix composites by a precursor infiltration
US5110771A (en) Method of forming a precracked fiber coating for toughening ceramic fiber-matrix composites
US5338598A (en) Sintered inorganic composites comprising co-sintered tape reinforcement
US7919039B2 (en) Ceramic fiber composite material
WO1993020024A1 (fr) Procede de fabrication de materiaux composites renforces par des fibres
EP2650272A1 (fr) Matériau composite à base d'oxyde
She et al. Reaction‐Bonded Three‐Layer Alumina‐Based Composites with Improved Damage Resistance
JPH1112050A (ja) 積層セラミックス及びその製造方法
US5567518A (en) Ceramic composite, particularly for use at temperatures above 1400 degrees celsius
US5425909A (en) Heat treatment for particle reinforced alumina ceramic composite
JP2002173376A (ja) 酸化物系セラミックス繊維/酸化物系セラミックス複合材料、及びその製造方法
US7105224B2 (en) Oxide ceramic fiber composite materials and use thereof
CN110981451B (zh) 一种含弹性结构界面的氧化物/氧化物陶瓷基复合材料的制备方法
JP2908309B2 (ja) セラミックス複合材料およびその製造方法
Pope et al. Laminated object manufacturing of Si3N4 with enhanced properties
US6624105B2 (en) Oxide ceramic fiber/oxide ceramic composite material and process for production thereof
董如林 et al. Influence of heat treatment on phases, microstructures and mechanical properties of laminated fabric (SiC and aluminosilicate)/mullite matrix composites
CA2135061C (fr) Composite en ceramique, notamment pour usage a des temperatures superieures a 1400.degre.c
Park et al. Fracture strength and damage resistance of slip cast Y-TZP/Ce-TZP layered composites
JPH05170522A (ja) アルミナ系複合セラミックス焼結体
Ma et al. Fracture behavior of ceramic layered systems with weak interlayers

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19990326

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): DE ES FR GB IT

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

17Q First examination report despatched

Effective date: 20001103

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): DE ES FR GB IT

REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

REF Corresponds to:

Ref document number: 69708682

Country of ref document: DE

Date of ref document: 20020110

ET Fr: translation filed
REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2164364

Country of ref document: ES

Kind code of ref document: T3

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IT

Payment date: 20160824

Year of fee payment: 20

Ref country code: DE

Payment date: 20160826

Year of fee payment: 20

Ref country code: GB

Payment date: 20160830

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20160825

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20160826

Year of fee payment: 20

REG Reference to a national code

Ref country code: DE

Ref legal event code: R071

Ref document number: 69708682

Country of ref document: DE

REG Reference to a national code

Ref country code: GB

Ref legal event code: PE20

Expiry date: 20170810

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20170810

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20180508

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20170812